US3779816A - Method of making mold for forming objects - Google Patents

Method of making mold for forming objects Download PDF

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Publication number
US3779816A
US3779816A US00175122A US3779816DA US3779816A US 3779816 A US3779816 A US 3779816A US 00175122 A US00175122 A US 00175122A US 3779816D A US3779816D A US 3779816DA US 3779816 A US3779816 A US 3779816A
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United States
Prior art keywords
titanium
mold
oxide layer
temperature
rate
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US00175122A
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English (en)
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G Mao
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GNB Inc
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Gould Inc
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Publication of US3779816A publication Critical patent/US3779816A/en
Assigned to GNB BATTERIES INC. reassignment GNB BATTERIES INC. ASSIGNMENT OF ASSIGNORS INTEREST. Assignors: GOULD INC.,
Assigned to CITIBANK, N.A. reassignment CITIBANK, N.A. SECURITY INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: GNB BATTERIES INC.
Assigned to GNB INCORPORATED reassignment GNB INCORPORATED RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: CITIBANK, N.A.
Assigned to GNB INCORPORATED reassignment GNB INCORPORATED RELEASED BY SECURED PARTY (SEE DOCUMENT FOR DETAILS). Assignors: CITIBANK, N.A.
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C23/00—Tools; Devices not mentioned before for moulding
    • B22C23/02—Devices for coating moulds or cores
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C3/00—Selection of compositions for coating the surfaces of moulds, cores, or patterns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D17/00—Pressure die casting or injection die casting, i.e. casting in which the metal is forced into a mould under high pressure
    • B22D17/20—Accessories: Details
    • B22D17/22—Dies; Die plates; Die supports; Cooling equipment for dies; Accessories for loosening and ejecting castings from dies
    • B22D17/2209—Selection of die materials

Definitions

  • ABSTRACT A mold for forming objects such as battery grids includes a cavity having a titanium layer with an adherent titanium oxide layer integrally formed thereon.
  • the oxide layer is formed by heating the titanium layer under controlled oxidizing conditions to provide an oxide layer of a specified thickness which is tenaciously adherent to the unoxidized titanium.
  • Cast iron is the typical material used for such molds but does not adequately satisfy the requirements identified herein; and, for this reason, it is conventional practice to coat battery grid molds with various types of coatings in an attempt to provide the necessary mold surface characteristics for the grid casting operation.
  • a widely used coating composition for gravity-type molds includes cork dust and clay suspended in water and sodium silicate.
  • a mold release agent such as silicone grease is generally required for each casting cycle. While such compositions function in an adequate manner, the frequency with which they must be reapplied (every three or four hours in the case of gravity-type mold coats) significantly reduces the attainable production rate.
  • a related object lies in the provision of a mold thatmay be used for a long period, in relation to presently used molds, without requiring interruption of casting to treat the mold surface to restore the necessary properties for casting.
  • Yet another object provides a mold having a surface which allows the formed object to be readily removed therefrom following the casting operation.
  • a further object of the present invention is to provide a mold having a surface which enhances the physical and chemical properties of the cast object.
  • a relatedwhich is capable of providing improved production rates and reduced downtime.
  • FIG. 1 is a photomicrograph (56X amplification) of part of the surface of a mold in accordance with the wssmit lt o
  • FIG. 2 is another photornicro'graph (Z Z SUX amplification) and illustrating, in cross section fashion, a portion of the surface of the mold shown in FIG. 1; and
  • FIG. 3 is a perspective view and showing a typical mold according to the present invention which can be employed in the casting of battery grids.
  • the present invention is directed to a mold with a titanium surface which has been treated under specified conditions to form an integral titanium oxide layer thereon which is tenaciously adherent to the remainder of the titanium.
  • the oxide layer formed in accordance with the method described herein, provides the mold with characteristics which allow use in forming operations without the necessity of coating the mold as is conventionally required.
  • the surface is desirably first cleaned by any conventional means, such as polishing or the like.
  • the titanium layer is then heated in an oxidizing atmosphere to provide an oxide layer on the titanium surface which is sufficient to provide the heat-insulating properties and other characteristics needed for forming but which is also tenaciously adherent to the remainder of the titanium. so as to provide a mold with excellent life for casting applications. Absent any mechanical damage, as by excessively scraping the surface to destroy the finish and/or its adherence or exposure to too high temperatures, the life of a mold made according to the present invention would be virtually without limit.
  • the temperature level of the titanium mold is desirably raised to from about 1200 to about l500F. at a rate which substantially prevents the development of thermal shock in the oxide layer being built up that would substantially lessen its adherence.
  • Temperatures below 1200F. can be employed but generally do not allow development of a layer of adequate thickness within acceptable time limits whereas temperatures above 1500F. begin to adversely affect the adherence of the titanium oxide layer to the titanium, and also create warpage of the tita-' nium.
  • Raising the temperature at a rate of from about 100F. per hour to about 200F. per hour will be a sufficiently slow rate to prevent undesirable thermal shock in most applications.
  • the temperature should be maintained at the maximum level for the time necessary to build up an oxide layer of sufficient thickness to satisfy the heatinsulating requirements of the particular forming operation involved. Thickness of about 0.25 to about 0,5 mil in thickness have been found suitable for battery grid casting. Thicknesses less than about 0.25 mil will generally possess inadequate properties for casting whereas thicknesses greater than about 0.5 mil tend to yield oxide layers with poor adhesion characteristics. Typically, a sufficient thickness for battery grid casting will be built up after a period of about 16 hours. It is hypothesized that the temperature of the titanium should not be varied to any significant extent once the maximum temperature has been reached because it is believed that such variation would prevent the formation of the monomorphic character of the oxide layer, which may well contribute to its ability to tightly adhere to the unoxidized portion.
  • the mold should desirably be completely supported in a flat position during the heating step to prevent warpage. This is particularly important when the temperatures being employed are in the higher part of the range. Any conventional type of furnace may be employed for heating, but the furnace should be bumed out or cleaned to prevent contamination during heating which could impair the adhesion characteristics of the oxide layer.
  • the type of oxidizing atmosphere which is employed is not particularly critical; however, it is advantageous to use a gas stream having a definite amount of the oxidizing agent since this simplifies control over the operation. However, if desired and with proper control, even the still air in a furnace or other heating chamber could be used.
  • the heated mold is thereafter cooled at a controlled rate which is slow enough to prevent any significant thermal shock which would, as was the case in the heating step, dissipate the adhesion levels of the oxide layer to the unoxidized titanium. Cooling at a rate of from about l to about 400F. per hour may be used under most conditions without impairing adhesion.
  • the oxide layer is subjected to a second heat treatment at a lower temperature to improve the adhesion of the oxide layer to the unoxidized titanium.
  • the mold is partially cooled at a rate to avoid thermal shock (e.g. l00 to 600F./hr. has been found satisfactory) and is then held at the intermediate temperature for a certain period of time.
  • this second heat treatment results in oxygen diffusion from the oxide layer to the interface between that layer and the unoxidized titanium which, in effect, improves the cohesiveness of these two layers at their interface. Accordingly, this second step should be carried out by cooling to a temperature and holding for a time adequate to effect the necessary oxygen diffusion or increase in adhesion.
  • the twice-heated mold may then be cooled at a rate of from about 100 to about 400F. per hour, which rates are satisfactory under most conditions to prevent the development of any significant amount of thermal shock.
  • the resulting mold as can be seen in the amplified photographs identified as FIGS. 1 and 2, comprises an unoxidized portion 10 with an oxide layer 12.
  • the oxide layer is tenaciously adherent to the unoxidized titanium.
  • tenaciously adherent it is meant that the formed layer is sufficiently adherent to withstand the operating conditions encountered in the forming or casting operations, typically for a long time in relation to presently used mold coats.
  • FIG. 3 shows a mold section formed from titanium treated as herein described which may be used in battery grid casting.
  • the mold section 20 comprises a gate area 22 and a cavity, shown generally at 24.
  • Examples 1 and 2 employed a rodof commercially pure titanium metal with a sample size and shape selected to simulate the cavities of a battery grid casting mold.
  • a titanium rod one-eighth inch in diameter and 3 inches in length was used with three one-eighth inch grooves machined near one end and having a diameter of about 1/16 inch. Diffraction techniques indicate that the oxide layer is Ti0 (Rutile form).
  • EXAMPLE l A specimen rod was cleaned by employing a polish consisting of, by volume, 10 parts hydrofluoric acid, 60 parts of a 30% aqueous hydrogen peroxide solution and 30 parts distilled water. The sample was cleaned for about 2 minutes.
  • the specimen was heated from ambient conditions to a temperature of about 1400F. with the heating being carried out at a rate of about 175F. per hour in an atmosphere of, by volume, argon and 5% oxygen in a Lindberg tube furnace.
  • the argon-oxygen stream was passed through the furnace at a rate of about 1 cu. ft./hr.
  • the temperature was held at 1400F. for l6 hours to provide the initial oxide layer.
  • a second heat treatment was then carried out in which the temperature was cooled after the first stage from 1400F. to l200F. at a rate of 600F. per hour and was held at l200F. for 16 hours while maintaining a vacuum of about 5 X l0"mm. mercury. Thereafter cooling to ambient conditions was carried out at a rate of about 400F. per hour.
  • the specimen achieved a gain in weight of about 158 X 10' grams per square centimeter, and this corresponded to an oxide layer of about 0.3 mils in thickness.
  • the oxide layer has very good adhesion and breaks off into only small pieces when subjected to extensive bending.
  • EXAMPLE 2 The specimen was treated with the polish described in Example 1 and, thereafter, was heated to a temperature of 1500F. from ambient conditions at a rate of 175F. per hour in a vacuum atmosphere (5 X 10"mm. mercury) in the furnace described in Example 1. The temperature was held at l500F. for 16 hours after which the specimen was cooled to ambient conditions at a rate of F. per hour.
  • a weight gain of 204 X 10 grams per square centimeter was obtained (i.e. -0.4 mils in thickness), and the oxide layer was tenaciously adherent to the unoxi- EXAMPLE 3
  • Example 2 e.g. -heated to 1500F. in a vacuum atmosphere of 5 X *mm. mercury, held at that temperature for 16 hours and cooled to ambient conditions at a rate of 100F. per hour.
  • the resulting oxide layer resisted repeated scratching with a sharp point.
  • the formed mold was placed in a conventional low pressure casting machine, and over 2000 calcium-lead grids (0.06% by weight calcium) were cast. The oxide layer survived this run, and the formed grids were easily removed from the mold. Microstructures of crosssections of a typical grid showed that the grain size was fairly uniform when compared with that of grids formed in a cast iron mold.
  • EXAMPLE 4 A tubular industrial grid mold with titanium inserts (one for the gate area and one for the mold cavity) were made by cleaning the surface of the inserts (as in Example 3) and thereafter forming an oxide layer thereon by treating the inserts as in Example 3.
  • the inserts were then bolted to a mold base to form a cavity with dimensions of: length -18 3 4 inches, width 5 7a inches, depth -3/l6 inch and with 14 splines.
  • the mold with the titanium inserts was installed in a conventional low pressure casting machine and used to form antimony-lead grids (7% by weight antimony). Casting qualities were satisfactory, the mold filled well; and the cast grids were easily removed. Grids could be cast satisfactorily at rates of about 78 per minute period.
  • the present invention provides a mold with a titanium layer and an integral oxide layer which has desirable properties when used in forming applications, such as casting lead-alloy battery grids.
  • the oxide layer is formed in accordance with the method ofthis invention, the layer is tenaciously adherent to the unoxidized portion and is capable of being used in molding operations for extended periods of time.
  • the release characteristics are such that the cast object suchas battery grids may be readily released or separated from the mold.
  • the oxide layer imparts desirable properties in the cast object; and, thus, castings may be obtained which have a smooth surface finish with desirable corrosion resistance.
  • the oxide layer has a thickness of only 0.25 to 0.5 mils so as to allow formation of cast objects of more uniform tolerances.
  • a method of making a mold for forming objects from a fluid comprising heating in an oxidizing atmosphere at least the titanium surface to raise the titanium to a temperature in the range of from about l200 to 1500? and to hold it for a time sufficient to oxidize the titanium surface to form an oxide layer which is adherent to the unoxidized titanium and with a thickness of about 0.25 to 0.5 mils which is sufficient to provide the necessary heat-insulating properties for the forming of the object and thereafter cooling the mold, the heating and cooling being carried out at rates controlled to substantially avoid thermal shock in the oxide layer.
  • a method of making a mold for forming objects from a fluid comprising heating in an oxidizing atmosphere the titanium surface to raise the titanium to a temperature in the range of from about 1200 to l500F. and to hold it for a time sufficient to oxidize the titanium surface to form an oxide layer which is adherent to the unoxidized titanium and with a thickness at least sufficient to provide the necessary heatinsulating properties for the forming of the object and thereafter cooling the mold, the heating and cooling being carried out at rates controlled to substantially avoid thermal shock in the oxide layer.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Molds, Cores, And Manufacturing Methods Thereof (AREA)
  • Moulds For Moulding Plastics Or The Like (AREA)
  • Mold Materials And Core Materials (AREA)
  • Cell Electrode Carriers And Collectors (AREA)
US00175122A 1971-08-26 1971-08-26 Method of making mold for forming objects Expired - Lifetime US3779816A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US17512271A 1971-08-26 1971-08-26

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Country Status (8)

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US (1) US3779816A (fr)
JP (1) JPS5528775B2 (fr)
BE (1) BE788005A (fr)
DE (1) DE2241685A1 (fr)
FR (1) FR2150544B1 (fr)
IT (1) IT964269B (fr)
LU (1) LU65952A1 (fr)
NL (1) NL7211673A (fr)

Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3972367A (en) * 1975-06-11 1976-08-03 General Electric Company Process for forming a barrier layer on ceramic molds suitable for use for high temperature eutectic superalloy casting
US4027716A (en) * 1974-03-11 1977-06-07 Metallgesellschaft Aktiengesellschaft Method for preparing a continuous casting belt
US4031945A (en) * 1976-04-07 1977-06-28 General Electric Company Process for making ceramic molds having a metal oxide barrier for casting and directional solidification of superalloys
US4120930A (en) * 1974-08-08 1978-10-17 Lemelson Jerome H Method of coating a composite mold
US4178981A (en) * 1978-06-29 1979-12-18 Kerr-Mcgee Corporation Copper casting method using titanium dioxide release method
US4263060A (en) * 1973-11-09 1981-04-21 Centre Stephanois De Recherches Mecanique Hydromecanique Et Frottement Method for treating parts made of titanium or titanium alloy, and parts produced thereby
US5287910A (en) * 1992-09-11 1994-02-22 Howmet Corporation Permanent mold casting of reactive melt
US5415219A (en) * 1992-07-21 1995-05-16 Hagen Batterie Ag Grid casting mold for the casting of lead grids for accumulators and methods for its manufacture
US5505246A (en) * 1994-06-17 1996-04-09 Howmet Corporation Permanent mold or die casting of titanium-aluminum alloys
US5989749A (en) * 1997-11-26 1999-11-23 Johnson Controls Technology Company Stamped battery grid
US6203948B1 (en) 1997-11-26 2001-03-20 Johnson Controls Technology Company Stamped grid having offset horizontal wires
US6245462B1 (en) 1999-05-20 2001-06-12 Johnson Controls Technology Company Battery grid and method of making
US6376022B1 (en) * 1998-05-14 2002-04-23 Southwest Research Institute Protective coating and method
US7767347B2 (en) 2005-05-23 2010-08-03 Johnson Controls Technology Company Battery grid
US8252464B2 (en) 1999-07-09 2012-08-28 Johnson Controls Technology Company Method of making a battery grid
US8586248B2 (en) 2010-04-14 2013-11-19 Johnson Controls Technology Company Battery, battery plate assembly, and method of assembly
US9130232B2 (en) 2010-03-03 2015-09-08 Johnson Controls Technology Company Battery grids and methods for manufacturing same
US9577266B2 (en) 2007-03-02 2017-02-21 Johnson Controls Technology Company Negative grid for battery
US9748578B2 (en) 2010-04-14 2017-08-29 Johnson Controls Technology Company Battery and battery plate assembly
US10170768B2 (en) 2013-10-08 2019-01-01 Johnson Controls Autobatterie Gmbh & Co. Kgaa Grid assembly for a plate-shaped battery electrode of an electrochemical accumulator battery
US10418637B2 (en) 2013-10-23 2019-09-17 Johnson Controls Autobatterie Gmbh & Co. Kgaa Grid arrangement for plate-shaped battery electrode and accumulator
US10892491B2 (en) 2011-11-03 2021-01-12 CPS Technology Holdings LLP Battery grid with varied corrosion resistance
US12132209B2 (en) 2022-12-21 2024-10-29 Cps Technology Holdings Llc Battery grid with varied corrosion resistance

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5245605B2 (fr) * 1973-05-09 1977-11-17
JPS5187419A (ja) * 1975-01-30 1976-07-31 Furukawa Electric Co Ltd Igatanohyomenshoriho
JPS55161545A (en) * 1979-06-01 1980-12-16 Matsushita Electric Ind Co Ltd Mold for lead storage battery grid
WO1983003212A1 (fr) * 1982-03-15 1983-09-29 Schmitt, Reimar Moule pour la coulee d'objets de faible epaisseur en metal ou en alliage a bas point de fusion, et procede de recouvrement de la surface active de ce moule

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2881105A (en) * 1957-10-17 1959-04-07 Chicago Dev Corp Method of fabricating and treating titanium-aluminum alloy parts to improve them forhigh temperature use
US3408236A (en) * 1964-07-16 1968-10-29 Hoover Ball & Bearing Co Wear-resistant titanium alloy and method of producing same
US3629388A (en) * 1970-01-12 1971-12-21 Rosanne A Levitsky Casting procedure for high quality epoxy layers

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2881105A (en) * 1957-10-17 1959-04-07 Chicago Dev Corp Method of fabricating and treating titanium-aluminum alloy parts to improve them forhigh temperature use
US3408236A (en) * 1964-07-16 1968-10-29 Hoover Ball & Bearing Co Wear-resistant titanium alloy and method of producing same
US3629388A (en) * 1970-01-12 1971-12-21 Rosanne A Levitsky Casting procedure for high quality epoxy layers

Cited By (35)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4263060A (en) * 1973-11-09 1981-04-21 Centre Stephanois De Recherches Mecanique Hydromecanique Et Frottement Method for treating parts made of titanium or titanium alloy, and parts produced thereby
US4027716A (en) * 1974-03-11 1977-06-07 Metallgesellschaft Aktiengesellschaft Method for preparing a continuous casting belt
US4120930A (en) * 1974-08-08 1978-10-17 Lemelson Jerome H Method of coating a composite mold
US3972367A (en) * 1975-06-11 1976-08-03 General Electric Company Process for forming a barrier layer on ceramic molds suitable for use for high temperature eutectic superalloy casting
US4031945A (en) * 1976-04-07 1977-06-28 General Electric Company Process for making ceramic molds having a metal oxide barrier for casting and directional solidification of superalloys
US4178981A (en) * 1978-06-29 1979-12-18 Kerr-Mcgee Corporation Copper casting method using titanium dioxide release method
US5415219A (en) * 1992-07-21 1995-05-16 Hagen Batterie Ag Grid casting mold for the casting of lead grids for accumulators and methods for its manufacture
US5443111A (en) * 1992-09-11 1995-08-22 Howmet Corporation Permanent mold for casting reactive melt
WO1995022423A1 (fr) * 1992-09-11 1995-08-24 Howmet Corporation Moulage de fonte reactive en coquille
US5287910A (en) * 1992-09-11 1994-02-22 Howmet Corporation Permanent mold casting of reactive melt
US5505246A (en) * 1994-06-17 1996-04-09 Howmet Corporation Permanent mold or die casting of titanium-aluminum alloys
US5989749A (en) * 1997-11-26 1999-11-23 Johnson Controls Technology Company Stamped battery grid
US6203948B1 (en) 1997-11-26 2001-03-20 Johnson Controls Technology Company Stamped grid having offset horizontal wires
US6376022B1 (en) * 1998-05-14 2002-04-23 Southwest Research Institute Protective coating and method
US6245462B1 (en) 1999-05-20 2001-06-12 Johnson Controls Technology Company Battery grid and method of making
US8252464B2 (en) 1999-07-09 2012-08-28 Johnson Controls Technology Company Method of making a battery grid
US8709664B2 (en) 1999-07-09 2014-04-29 Johnson Controls Technology Company Battery grid
US7955737B2 (en) 2005-05-23 2011-06-07 Johnson Controls Technology Company Battery grid
US8399135B2 (en) 2005-05-23 2013-03-19 Johnson Controls Technology Company Battery grid
US7767347B2 (en) 2005-05-23 2010-08-03 Johnson Controls Technology Company Battery grid
US8974972B2 (en) 2005-05-23 2015-03-10 Johnson Controls Technology Company Battery grid
US8980419B2 (en) 2005-05-23 2015-03-17 Johnson Controls Technology Company Battery grid
US9577266B2 (en) 2007-03-02 2017-02-21 Johnson Controls Technology Company Negative grid for battery
US9130232B2 (en) 2010-03-03 2015-09-08 Johnson Controls Technology Company Battery grids and methods for manufacturing same
US10985380B2 (en) 2010-04-14 2021-04-20 Cps Technology Holdings Llc Battery and battery plate assembly with highly absorbent separator
US9748578B2 (en) 2010-04-14 2017-08-29 Johnson Controls Technology Company Battery and battery plate assembly
US8586248B2 (en) 2010-04-14 2013-11-19 Johnson Controls Technology Company Battery, battery plate assembly, and method of assembly
US11824204B2 (en) 2010-04-14 2023-11-21 Cps Technology Holdings Llc Battery and battery plate assembly with absorbent separator
US10892491B2 (en) 2011-11-03 2021-01-12 CPS Technology Holdings LLP Battery grid with varied corrosion resistance
US11539051B2 (en) 2011-11-03 2022-12-27 Cps Technology Holdings Llc Battery grid with varied corrosion resistance
US10170768B2 (en) 2013-10-08 2019-01-01 Johnson Controls Autobatterie Gmbh & Co. Kgaa Grid assembly for a plate-shaped battery electrode of an electrochemical accumulator battery
US10840515B2 (en) 2013-10-08 2020-11-17 Clarios Germany Gmbh & Co. Kgaa Grid assembly for a plate-shaped battery electrode of an electrochemical accumulator battery
US11611082B2 (en) 2013-10-08 2023-03-21 Clarios Germany Gmbh & Co. Kg Grid assembly for a plate-shaped battery electrode of an electrochemical accumulator battery
US10418637B2 (en) 2013-10-23 2019-09-17 Johnson Controls Autobatterie Gmbh & Co. Kgaa Grid arrangement for plate-shaped battery electrode and accumulator
US12132209B2 (en) 2022-12-21 2024-10-29 Cps Technology Holdings Llc Battery grid with varied corrosion resistance

Also Published As

Publication number Publication date
FR2150544A1 (fr) 1973-04-06
NL7211673A (fr) 1973-02-28
IT964269B (it) 1974-01-21
BE788005A (fr) 1972-12-18
JPS4831125A (fr) 1973-04-24
FR2150544B1 (fr) 1978-04-14
LU65952A1 (fr) 1973-01-15
JPS5528775B2 (fr) 1980-07-30
DE2241685A1 (de) 1973-03-01

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Owner name: GNB BATTERIES INC., 1110 HIGHWAY 110, MENDOTA HEIG

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Effective date: 19840106

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Owner name: CITIBANK, N.A. 641 LEXINGTON AVENUE NEW YORK NY 10

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Effective date: 19871021